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Trifluoroacetic acid → HCID 178501913、化合物

HRID 1488051
ノート
印刷プレビュー

反応式

HRID 1488051 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:12][N:11]([C:13]([C:15]3[CH:16]=[CH:17][C:18]([CH3:40])=[C:19]([C:21]4[N:22]=[C:23]([CH:27]5[CH2:32][CH2:31][N:30]([C:33]([O:35][C:36](C)(C)C)=[O:34])[CH2:29][CH2:28]5)[NH:24][C:25]=4[CH3:26])[CH:20]=3)=[O:14])[CH2:10]2)=[CH:5][CH:4]=1)#[N:2].FC(F)(F)C(O)=O.CC1C=CC(C(N2CC(C3C=CC(C#N)=CC=3)C2)=O)=CC=1C1NC(C2CCNCC2)=NC=1C.C(N(C(C)C)CC)(C)C.ClC(OC)=O>C(Cl)Cl.CN(C=O)C>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:10][N:11]([C:13]([C:15]3[CH:16]=[CH:17][C:18]([CH3:40])=[C:19]([C:21]4[NH:22][C:23]([CH:27]5[CH2:32][CH2:31][N:30]([C:33]([O:35][CH3:36])=[O:34])[CH2:29][CH2:28]5)=[N:24][C:25]=4[CH3:26])[CH:20]=3)=[O:14])[CH2:12]2)=[CH:5][CH:4]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6422Trifluoroacetic acidHCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 90021783t-Butyl 4-(4-(5-(3-(4-cyanophenyl)azetidine-1-carbonyl)-2-methylphenyl)-5-methyl-1H-imidazol-2-yl)piperidine-1-carboxylate2 回HCID 178425785HCID 178425785、化合物

生成物 1

HCID 178501913
HCID 178501913、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 4-(4-(5-(3-(4-cyanophenyl)azetidine-1-carbonyl)-2-methylphenyl)-5-methyl-1H-imidazol-2-yl)piperidine-1-carboxylate (compound 182.3, 227 mg, 0.42 mmol) in CH2Cl2 (10 mL), was added trifluoroacetic acid (2 ml). The reaction was stirred for 1.5 hours and concentrated under reduced pressure. The reaction mixture was neutralized with 2 mL Na2CO3 (1M) to afford the crude intermediate after lyophilization. A mixture of 4-(1-(4-methyl-3-(4-methyl-2-(piperidin-4-yl)-1H-imidazol-5-yl)benzoyl)azetidin-3-yl)benzonitrile (185 mg, 0.42 mmol) and diisopropyl ethylamine (363 μL, 2.1 mmol) were dissolved in DMF (6 mL). Methyl chloroformate (36 μL, 0.46 mmol) was added and the mixture was stirred at room temperature for 1 hour. The reaction was concentrated, diluted with saturated NaH2PO4 (20 mL) and extracted with EtOAc (3×20 ml). The organic phase was washed by brine, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by preparative TLC with 10% methanol in dichloromethane and lyophilized to give 141 mg (67%, over 2 steps) of the title compound as a white solid. m/z (ES+) 498 (M+H)+.

後処理

  1. concentrationconcentrated under reduced pressure
  2. customto afford the crude intermediate after lyophilization
  3. stirringthe mixture was stirred at room temperature for 1 hour
  4. concentrationThe reaction was concentrated
  5. additiondiluted with saturated NaH2PO4 (20 mL)
  6. extractionextracted with EtOAc (3×20 ml)
  7. washThe organic phase was washed by brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was purified by preparative TLC with 10% methanol in dichloromethane

出典と根拠

ORDレコード
ord-613e34392c694443a61ee5f22797fdb8
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428502B2

反応ノート

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